CN1510700A - R-Fe-B sintered magnet containing trace oxygen and method for producing same - Google Patents
R-Fe-B sintered magnet containing trace oxygen and method for producing same Download PDFInfo
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- CN1510700A CN1510700A CNA021587078A CN02158707A CN1510700A CN 1510700 A CN1510700 A CN 1510700A CN A021587078 A CNA021587078 A CN A021587078A CN 02158707 A CN02158707 A CN 02158707A CN 1510700 A CN1510700 A CN 1510700A
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 43
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000001301 oxygen Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000003801 milling Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims 2
- 229910052779 Neodymium Inorganic materials 0.000 claims 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- 229910052691 Erbium Inorganic materials 0.000 claims 1
- 229910052689 Holmium Inorganic materials 0.000 claims 1
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- 229910052775 Thulium Inorganic materials 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 229910052735 hafnium Inorganic materials 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 229910052758 niobium Inorganic materials 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 229910052715 tantalum Inorganic materials 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 238000005259 measurement Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000006213 oxygenation reaction Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 208000018875 hypoxemia Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention belongs to the field of permanent magnetic RE material. Mainly relates to a high-quality R-Fe-B sintered magnet and a method for producing the same. Using an inert atmosphere (including N) during the manufacturing process2Atmosphere), controlling the oxygen content in the magnet within the range of 100-1200 ppm to obtain a high-quality sintered R-Fe-B magnet with excellent uniformity, and after airflow milling classification, directly using ultrafine powder with the particle size of less than 2 microns to prepare the high-quality R-Fe-B magnet, wherein the material utilization rate is improved by 10-20%, and the economic benefit is obvious.
Description
Technical field the invention belongs to the rare earth permanent-magnetic material field.Relate generally to high-quality sintering R-Fe-B series magnet and manufacture method thereof.
The high-quality R-Fe-B series magnet of background technology can make magnet device miniaturization, lightweight, high performance, and in the last few years, its demand constantly increased, and the research and development of high-quality R-Fe-B series magnet are also quite paid attention to.
In the prior art, all oxygen is got rid of outside the magnet composition as the most harmful impurity element, three elemental gas H, N, F are included in the magnet composition at the patent US 5645651 of the U.S. in overdue Sumitomo Special Metal Co., Ltd in 2014, only not oxygen as the composition element.Nearly all first consideration of the oxygen content in the reduction magnet as technological design, along with the reduction of oxygen content, magnet performance improves constantly all R-Fe-B series magnet production technologies.At present dry process and damp process of adopting are made sintering R-Fe-B based sintered magnet more.SUMITOMO CHEMICAL particulate metal Co., Ltd. adopts dry process (Fig. 1): 1 raw material → 2 cast scale → 3 hydrogen and pulverize mill → 5 airflow milling → 6 batch mixings → 7 known technology moulding → 8 sintering → 9 timeliness in → 4 → 10 processing, detect.Adopt methods such as antioxidant, dispersant, lubricant at break section, realized reducing the purpose of oxygen content in the production process, and adopt known, inertialess atmosphere (to comprise N
2Interior) protection forming technique produced high-quality magnet.But oxygen content is low inadequately and decentralization is big, and its oxygen content is seen Japan Patent No. 3231034 in the scope of 2900ppm～5300ppm.
Hitachi Metal Co., Ltd. adopts wet process (mineral oil is made the protection medium), has obtained the high-quality R-Fe-B series magnet of hypoxemia, and oxygen content is at 1200ppm～2000ppm (between 0.12～0.20wt%) in the magnet.See Japan Patent (spy opens flat 11-97223).But manufacturing process complexity, operation various (as the de-oiling operation must be arranged) etc.
In addition, use the industrial production of the dry method manufacturing sintering R-Fe-B series magnet of present technology to be difficult to realize oxygen content is reduced to below the 1200ppm.
The summary of the invention prior art all oxygen as a kind of harmful element, when producing high-quality rare earth magnet, reduce its content in rare earth magnet, because its oxygen content of technical problem always greater than 1500ppm, is not therefore found the beneficial effect of oxygen as far as possible.The present invention adopts the ZHOFP technology of controlled oxygenation, and after the content of oxygen in magnet was less than 1000ppm (0.1wt%), the illeffects of oxygen had been reduced to insignificant, particularly reduces to 800ppm when following, and this moment, oxygen just obviously rose to the advantageous effect of magnet.The present invention makes up, transforms by the equipment from the smelting engineering to the overall process of sintering engineering, and adopts positive extra large anaerobic technology (ZHOFP) technology, has realized the industrial production of the R-Fe-B permanent magnet under oxygen-free environment.The production procedure of ZHOFP (Fig. 2) is: 1 raw material → 2 cast scale → 3 hydrogen and pulverize → 4 ' middle mill (controlled oxygenation) → 5 airflow milling → 6 batch mixings → 7 ' anaerobic (O
2≈ 0) moulding → 8 sintering → 9 timeliness in the environment → 10 processing, detect.Oxygen content in the magnet is less than 1200ppm, and can be controlled in 100～400ppm, in the scope of 400～800ppm and 800～1200ppm, produces the high-quality R-Fe-B magnet that contains micro amount of oxygen of different brackets.
Owing to adopted special oriontation shaping device of the present invention, realized being crushed to the oxygen-free environment of the whole Flow of Goods and Materials process of sintering furnace from hydrogen, stoped combining of oxygen and magnet powder, the oxygen content that makes final sintered magnet is less than 1200ppm, by special oxygen amount control, can in magnet, add oxygen element, realize 100ppm＜O＜400ppm, the adding of oxygen element in the magnet of 400ppm＜O＜800ppm and 800ppm＜O＜1200ppm.
The R-Fe-B series magnet that contains micro amount of oxygen of the present invention has following advantage:
1, the total amount of rare earth in the magnet greater than 28wt%, has reduced the consumption of expensive total amount of rare earth less than 29wt%.Particularly the consumption of heavy rare earth has reduced 30～50%.
2, produce (BH) max=400KJ/m easily
3(50MGOe) Yi Shang high-quality R-Fe-B series magnet.
3, reduce sintering temperature significantly, can carry out sintering 800 ℃～1050 ℃ temperature.
4, corrosion resistance improves.
5, can directly be fired into high-quality magnet with the superfines of particle mean size＜2 μ m after the airflow milling classification, without timeliness, simplified technology, and the varigrained powder of airflow milling is rationally used, the utilance of airflow milling powder improves 10～20%, greatly reduces cost.
Embodiment 1～8
According to sintered magnet composition (percentage by weight) Nd
21-xPr
8Dy
xCo
2.5Cu
0.2Ga
0.2B
1Nb
0.2Fe
Surplus(x=0～8), earlier the raw material of purity greater than 99wt% are prepared in proportion, fusing in 500kg/ time Strip casting (strip casting) smelting furnace, linear velocity with the running roller of per second 0.5～5m/s, carry out the scale casting, finally obtain the thick scale of 0.2～0.5mm, send into continous way hydrogen pulverization process stove and carry out the hydrogen pulverizing.At first under the Hydrogen Vapor Pressure of 90kPa, inhaled hydrogen 1～4 hour, vacuum dehydrogenation 6～8 hours in 200 ℃ of true temperature ranges of 0 ℃ then, reach below the 10Pa, cooled off at last 6～8 hours, the mill pulverizer was pulverized during particle after hydrogen is pulverized was sent under oxygen-free environment, and in middle mill process, controlledly add oxygen element by the present invention, final oxygen content with the control magnet, middle mill back particle＜0.5mm, enter airflow milling and carry out the broken and classification adjustment particle size distribution of micro mist, final acquisition distributed pole is narrow, the R-Fe-B powder that scope is adjustable, average grain diameter d=2～4 μ m enters inert atmosphere through oxygen-free environment and (comprises N
2Interior) the magnetic aligning moulding press of protection carries out moulding, and pressure 300～500kg/cm is automatically taken out in automatic feed
2, orientation field 2～6 * 10
4Oe, the oxygen concentration＜1000ppm in the press enters sintering furnace through oxygen-free environment at last, carry out the sintering of 800～1050 ℃ * 1～4hr, cold soon, carry out the Ageing Treatment of 900 ℃ * 1hr and 450～600 ℃ * 1～6hr then, take out, machine work is magnetized and is handled, and measurement result is shown in table 1.
The composition of table 1 magnet and magnetic characteristic
| Embodiment NO. | Magnet composition/wt% | ??Br/KG | ?jHc/KOe | ?(BH)max/ ???MGOe | |||
| ??Nd+Pr+Dy | ????O | ????C | ????N | ||||
| ????1 | ????28.34 | ??0.0764 | ??0.0233 | ??0.0595 | ???14.77 | ???14.66 | ???50.29 |
| ????2 | ????28.21 | ??0.0750 | ??0.0220 | ??0.0450 | ???14.45 | ???14.45 | ???50.50 |
| ????3 | ????28.05 | ??0.0738 | ??0.0232 | ??0.0594 | ???14.39 | ???15.35 | ???49.44 |
| ????4 | ????28.05 | ??0.0735 | ??0.0232 | ??0.0594 | ???14.38 | ???15.35 | ???49.53 |
| ????5 | ????28.21 | ??0.0272 | ??0.0392 | ??0.0436 | ???14.78 | ???12.43 | ???51.6 |
| ????6 | ????28.41 | ??0.0280 | ??0.0392 | ??0.0436 | ???14.64 | ???12.92 | ???51.46 |
| ????7 | ????28.27 | ??0.0250 | ??0.0340 | ??0.0506 | ???14.39 | ???13.46 | ???49.36 |
| ????8 | ????28.67 | ??0.0367 | ??0.0338 | ??0.0675 | ???14.46 | ???13.33 | ???50.30 |
As can be seen from Table 1, (730～770ppm) scopes can stably obtain the magnet (embodiment 1～4) of (BH) max 50MGOe, jHc ≈ 15kOe to Control for Oxygen Content, and Control for Oxygen Content can stably obtain the magnet (embodiment 5～8) of (BH) max 50MGOe, jHc ≈ 13kOe when (300ppm) about 0.0300wt% at 0.0730～0.0770wt%.Obviously by the inventive method, can make the good high-quality magnet of homogeneity as requested.
Embodiment 9～12
(760～270ppm), other are identical with embodiment 1～8 except that oxygen content being controlled at 0.0760wt% and 0.0270wt% respectively.Measurement result is shown in table 2.From table 1 and table 2 as can be seen, Control for Oxygen Content can obtain the high-quality magnet of height (BH) max, high rectangle degree (Hk/jHc) about 0.0700wt%.
The relation of table 2 oxygen content and Hk/jHc
| Embodiment NO. | ??O/wt％ | ?Br/KG | ?jHc/KOe | ?bHc/KOe | ??Hk/KOe | ??Hk/jHc | ?(BH)max/ ???MGOe |
| ????9 | ??0.0770 | ??14.38 | ???14.59 | ???13.52 | ???14.18 | ???0.97 | ???49.48 |
| ????10 | ??0.0750 | ??14.50 | ???14.54 | ???13.60 | ???14.06 | ???0.96 | ???50.35 |
| ????11 | ??0.0269 | ??14.33 | ???13.41 | ???12.04 | ???11.14 | ???0.83 | ???49.25 |
| ????12 | ??0.0280 | ??14.37 | ???13.58 | ???11.96 | ???11.16 | ???0.82 | ???49.51 |
Embodiment 13～16
Magnet is formed identical with embodiment 1～8, manufacturing process is also identical with embodiment 1～8, but the powder of making magnet is the superfine powder (accounting for total amount 10～20%) of the granularity d＜2 μ rm after the airflow milling classification, can control oxygen amount in the magnet less than 400ppm by technology of the present invention, this part fine powder can be sintered directly into magnet, and need not timeliness.Table 3 illustrates the sintering temperature and the magnetic characteristic of the sintered magnet that the superfine powder of utilizing granularity d＜2 μ m directly obtains.
The magnet performance that the fine powder of table 3 granularity d＜2 μ m sinters into
| Embodiment NO. | ??O/wt％ | Sintering temperature/℃ | ???Br/KG | ??jHc/KOe | ??(BH)max/ ????MGOe |
| ??13 | ??0.1000 | ????1000 | ????14.04 | ???14.15 | ????47.18 |
| ??14 | ??0.1040 | ????1000 | ????13.86 | ???15.48 | ????46.27 |
| ??15 | ??0.0980 | ????990 | ????12.81 | ???20.22 | ????38.96 |
| ??16 | ??0.0990 | ????990 | ????12.82 | ???20.06 | ????38.95 |
| Comparative example 1 | ??0.1500 | ????1060 | ????13.90 | ???16.50 | ????46.60 |
Comparative example 1
Magnet is formed with embodiment 1～8, and except that not adding the oxygen, other are identical with embodiment 1～8 with controlling.Measurement result also is shown in table 3.As can be seen from Table 3, adopt technology of the present invention, oxygen content within the scope of the present invention, in lower sintering temperature and with before out of use 10～15% superfine powder can make high-quality R-Fe-B series magnet, and the comparative example 1 of employing prior art, its oxygen content height, sintering temperature height and magnet performance are low.
Embodiment 17～20
Implementing process is the same, consists of (Nd
21-xPr
8Dy
x) Co
2.5Cu
0.2Ga
0.2B
1Nb
0.2Fe
Surplus, (x=0～8.0) adjust the x value, and Control for Oxygen Content in the scope of 100～400ppm, can be obtained high energy product, high-coercive force magnet, and measurement result is shown in table 4.As can be seen from Table 4, [(BH) max] numerical value+[jHc] numerical value 〉=66.
The high energy product of table 4, high-coercive force magnet
| Embodiment NO. | The x value | ??O/wt％ | ???Br/KG | ?jHc/KOe | ?(BH)max/MGOe |
| ????17 | ????1.2 | ??0.0260 | ???14.22 | ???17.0 | ????49.5 |
| ????18 | ????3.0 | ??0.0320 | ???13.60 | ???22.0 | ????45 |
| ????19 | ????6.0 | ??0.0280 | ???13.10 | ???26.0 | ????41.5 |
| ????20 | ????7.0 | ??0.0270 | ???12.3 | ???30.0 | ????37 |
Fig. 1 is current dry process a---process chart.Fig. 2 is through anaerobic technology---process chart.
Claims (6)
1, a kind of anisotropy sintering R-(Fe TM)-the B-X magnet, is characterised in that:
Wherein R refers among rare-earth elements La, Ce, Pr, Nd, Sm, Tb, Dy, Ho, Er, Tm, Y, the Lu etc. at least a kind;
20＜(Nd, Pr, Dy/Tb)＜and 30wt%, 0＜all the other rare earth element＜10wt%;
Among TM=Ti, V, Cr, Mn, Co, Ni, Ga, Ca, Cu, Zn, Si, Al, Mg, Zr, Nb, Hf, Ta, W, the Mo etc. at least a kind;
X＝N、C、H、O；
N＜3000ppm(0.3wt％)，C＜1000ppm(0.1wt％)，
H＜20ppm(0.002wt％)，100＜O＜1200ppm。
2, the Control for Oxygen Content in the magnet 100＜O＜400ppm (in the scope of 0.01＜O＜0.04wt%), (BH) max 〉=50MGOe, the jHc 〉=11KOe of magnet.
3, the Control for Oxygen Content in the magnet 400＜O＜800ppm (in the scope of 0.04＜O＜0.08wt%), (BH) max 〉=45MGOe, the jHc 〉=11KOe of magnet.
4, the Control for Oxygen Content in the magnet 800＜O＜1200ppm (in the scope of 0.08＜O＜0.12wt%), (BH) max 〉=40MGOe, the jHc 〉=11KOe of magnet.
5, in claim 1～4, (comprise N at inert atmosphere
2) the anaerobic technology (ZHOFP technology) of realization fully-automatic production in the protection oxygen-free environment down.
6, use in claim 1～4 after the airflow milling classification, the superfines that 2 μ m are following directly is fired into high-quality R-Fe-B magnet, without timeliness.
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|---|---|---|---|
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|---|---|
| CN1510700A true CN1510700A (en) | 2004-07-07 |
| CN1225750C CN1225750C (en) | 2005-11-02 |
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| WO2007053978A1 (en) * | 2005-11-10 | 2007-05-18 | Yantai Zhenghai Magnetic Material Co., Ltd. | R-Fe-B SYSTEM SINTER MAGNET COMPRISING MICROSCALE OXYGEN AND MANUFACTURING METHOD THEREOF |
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